Sonochemical Synthesis of Nanomaterials

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Sonochemical synthesis of nanomaterials

Cite this: Chem. Soc. Rev., 2013,
42, 2555
Hangxun Xu, Brad W. Zeiger and Kenneth S. Suslick*

High intensity ultrasound can be used for the production of novel materials and provides an unusual
route to known materials without bulk high temperatures, high pressures, or long reaction times.
Several phenomena are responsible for sonochemistry and specifically the production or modification of
nanomaterials during ultrasonic irradiation. The most notable eects are consequences of acoustic
cavitation (the formation, growth, and implosive collapse of bubbles), and can be categorized as
primary
sonochemistry
(gas-phase
chemistry
occurring
inside
collapsing
bubbles),
secondary
Received 26th July 2012
sonochemistry (solution-phase chemistry occurring outside the bubbles), and physical modifications
DOI: 10.1039/c2cs35282f
(caused by high-speed jets or shock waves derived from bubble collapse). This tutorial review provides
www.rsc.org/csr
examples of how the chemical and physical eects of high intensity ultrasound can be exploited for the
preparation or modification of a wide range of nanostructured materials.
1. Introduction
High intensity ultrasound has found many important applications
in organic synthesis, materials and organometallic chemistry, and
industrial manufacturing processes.19 Sonochemistry originates
from the extreme transient conditions induced by ultrasound,
which produces unique hot spots that can achieve temperatures
above 5000 K, pressures exceeding 1000 atmospheres, and heating
Department of Chemistry, University of Illinois at Urbana-Champaign, 600 South

Mathews Ave., Urbana, Illinois 61801, USA. E-mail: ksuslick@illinois.edu;
Fax: +1 217 333 2685; Tel: +1 217 333 2794
Part of the chemistry of functional nanomaterials themed issue.
Hangxun Xu
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Hangxun Xu was born in

Zhejiang, China, in 1983. He
obtained his BS degree in
polymer chemistry from the
University of Science and
Technology of China (USTC) in
2006. He then came to the
United States and received his
PhD in chemistry (2011, under
the supervision of Prof. Kenneth
S. Suslick) at the University of
Illinois at Urbana-Champaign
and is now a postdoctoral
research associate with Prof.
John A. Rogers.
The Royal Society of Chemistry 2013
and cooling rates in excess of 1010 K s1.4,10 These conditions are

distinct from other conventional synthetic techniques such as
photochemistry, wet chemistry, hydrothermal synthesis, or flame
pyrolysis (Fig. 1).24,11
The speed of sound in a typical liquid is 1000 to 1500 m s1,
and ultrasonic wavelengths will vary from roughly 10 cm down
to 100 mm over a frequency range of 20 kHz to 15 MHz, much
larger than the molecular size scale. The chemical and physical
eects of ultrasound therefore arise not from a direct interaction
between chemical species and sound waves, but rather from the
physical phenomenon of acoustic cavitation: the formation, growth,
and implosive collapse of bubbles.1113 When sound waves with
sucient amplitude propagate through a liquid, the liquid is
Brad W. Zeiger
Brad Zeiger received his BS in

chemistry
from
Western
Washington University in 2007,
where he studied complexes of
group VI metals with catecholate
ligands. He is currently pursuing
his PhD in inorganic chemistry at
the University of Illinois at UrbanaChampaign. His research has
focused on the physical and
chemical eects of ultrasound,
with specific interests including
sonocrystallization,
ultrasonic
processing of molecular crystals,
and time-resolved single-bubble
sonoluminescence.
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Fig. 2 Schematic illustration of the process of acoustic cavitation: the formation,

growth and implosive collapse of bubbles in a liquid irradiated with high intensity
ultrasound.
Fig. 1 Islands of chemistry as a function of time, pressure, and energy. Sonochemistry occupies a unique short-time, high-energy, and high-pressure space.
Reprinted with permission from ref. 10. Copyright 2008 Annual Reviews.
under dynamic tensile stress and the density changes with

alternating expansive and compressive waves. Bubbles will be
generated from pre-existing impurities (e.g., gas-filled crevices
in dust motes) and oscillate with the applied sound field. As
illustrated in Fig. 2, bubbles can grow through a slow pumping
of gas from the bulk liquid into the oscillating bubble (rectified
diusion). Bubbles at a critical size (usually tens of micrometres) can couple strongly to the acoustic field and undergo a
rapid inertial overgrowth during expansion, followed by a
catastrophic collapse. The implosive collapse process is nearly
adiabatic in its final stages and is responsible for the extreme
conditions characteristic of sonochemistry.
The extreme, transient conditions produced during acoustic
cavitation allow the formation of unique materials and also
permit syntheses on the benchtop in a room-temperature liquid
that would otherwise require high temperatures, high pressures,
or long reaction times. When a liquid is irradiated by high
Ken Suslick is the Marvin T.

Schmidt Professor of Chemistry
at the University of Illinois at
Urbana-Champaign.
Professor
Suslick received his BS from
Caltech in 1974, PhD from
Stanford in 1978. Suslick is the
recipient of the Sir George Stokes
Medal of the Royal Society of
Chemistry, the ACS Nobel
Laureate Signature Award for
Graduate Education, the MRS
Medal, the ACS Senior Cope
Kenneth S. Suslick
Scholar Award, the Mentorship
Award of the ASA, a Guggenheim Fellowship, and the Silver
Medal of the Royal Society for Arts. He is a Fellow of the AAAS,
ACS, MRS and ASA.
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Chem. Soc. Rev., 2013, 42, 2555--2567
intensity ultrasound, high-energy chemical reactions occur.

Sonochemistry can be employed in the synthesis of materials
from volatile or nonvolatile precursors, but generally through
dierent mechanisms (Fig. 3). In the former case, the volatile
precursor (e.g., a volatile organometallic compound) will produce
free metal atoms generated by bond dissociation due to the high
temperatures created during bubble collapse. These atoms can
be injected into the liquid phase and nucleate to form nanoparticles or other nanostructured materials if appropriate
templates or stabilizers are present in the solution. Nonvolatile
precursors may still undergo sonochemical reactions, even outside of the collapsing bubbles by undergoing reactions with
radicals or other high energy species produced from the sonolysis of vapour molecules inside the collapsing bubbles that then
diuse into the liquid phase to initiate a series of reactions
(e.g., reduction of metal cations).
The physical eects induced by high intensity ultrasound
are also often accompanied by chemical consequences and find
increasingly frequent use in materials synthesis. A trivial example
is the simple heating of the bulk liquid: typical laboratory scale
ultrasonic horns (Fig. 4) deliver roughly 10 to 100 watts of
Fig. 3 Primary sonochemistry and secondary sonochemistry for preparation of

nanomaterials. An example of primary sonochemistry is the generation of metal
atoms from sonolysis of weak metalcarbon bonds from volatile organometallic
compounds inside the collapsing bubble that then diuse into the bulk liquid to
form functional nanomaterials. Secondary sonochemical products may arise from
chemically active species (e.g., organic radicals from sonolysis of vapour) that are
formed inside the bubble, but then diuse into the liquid phase and subsequently react with solution precursors to form a variety of nanostructured
materials.
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Fig. 5 A spherical shock wave launched from a laser-induced collapsing bubble.

The shock wave can reach 60 kbar with velocities of 4 km s1. Images were
acquired at a shutter speed of 20.8 million frames per second, frame size was
1.5 1.8 mm2, and the exposure time was 5 ns. Reprinted with permission from
ref. 15. Copyright 1999 The Royal Society.
Fig. 4 A typical laboratory rig for sonochemical reactions uses a high intensity
ultrasonic horn, typically around 20 kHz and 10 to 100 W acoustic power.
Reprinted with permission from ref. 3. Copyright 2010 John Wiley & Sons.
acoustic energy into the liquid during sonication. This ultrasonic

power output must be calibrated, most commonly by calorimetry,
in order to accurately report experimental conditions, but
unfortunately many researchers overlook this critical parameter.
A common alternative to ultrasonic horns, ultrasonic cleaning
baths, are common in research labs and are easily obtained. The
actual ultrasonic power density of an ultrasonic cleaning bath is
typically only a few percent of that generated by an ultrasonic
horn. Cleaning baths are often marginal for many sonochemical
reactions, but can be useful for the physical eects of ultrasound,
e.g., for activating highly reactive metals (e.g., Li or Mg), generating
emulsions, accelerating dissolutions of solids, facilitating crystallizations, and exfoliating layered materials.
The most important physical phenomena for the preparation or modification of nanomaterials are microjets and shock
waves. Microjets occur when bubbles collapse near an extended
surface (i.e., surfaces several times larger than the bubble
radius).14 The inhomogeneity of the bubbles surroundings
induces an asphericity into the bubble, which self-reinforces
during collapse; this is similar to a shaped-charge explosive.
These high speed microjets impact on the surface and can
cause pitting and erosion of surfaces leading to modification of
surfaces and generation of surface nanostructures.
If the bubble is unperturbed by a surface, then the rapid
rebound from its minimum radius is spherical. The compression of the surrounding liquid propagates outward as a shock
wave from the rebounding bubble. A shock wave generated
from a laser-induced collapsing bubble is shown in Fig. 5.15 Such
shocks can reach pressures of 60 kbar and velocities of 4 km s1
in water. These shock waves can induce several dierent physical
eects with chemical consequences, including enhanced mass
transport due to strong turbulent mixing and acoustic streaming.
In addition, shock waves can accelerate solid particles suspended
in the liquid. Interparticle collisions can reach velocities of
hundreds of metres per second, causing changes in particle size
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distributions, particle morphologies, and surface compositions.16,17

Particle agglomeration (for malleable materials), particle fragmentation (for brittle materials) and exfoliation of layered materials into
2D layers have all been observed.2,3,9
The applications of high intensity ultrasound to materials
chemistry are diverse and rapidly increasing. Fig. 6 gives a
broad organizational schema for sonomaterials research to
date. In this tutorial review, we provide a sampling of the most
important and most recent results of sonochemical applications
to nanomaterials synthesis and preparation. We have organized
the review based on the chemical or physical eect of ultrasound
exploited for the formation of nanomaterials: (1) primary sonochemistry employing volatile precursors, (2) secondary sonochemistry using non-volatile precursors, (3) materials created
or modified through the physical eects of ultrasound (i.e.,
shock waves), and (4) materials in which both chemical and
physical eects of ultrasound have a synergistic impact.
2. Chemical eects of ultrasound for

nanomaterials preparation
A.
Nanomaterials prepared from volatile precursors
Ultrasonic irradiation of volatile organometallic compounds

such as Fe(CO)5 or Cr(CO)6 in a nonvolatile solvent (e.g.,
silicone oil or long-chain hydrocarbons) results in dissociation
of the metal-carbonyl bonds and release of individual elemental metal atoms.18 These atoms will be thermally excited to the
point that they emit visible light analogous to emission from
flame excitation and their atomic emission lines have been
used to characterize the bubble conditions.19 Nonvolatile solvents
are necessary because additional vapour, especially of polyatomics,
absorbs the available energy in the collapsing bubble (via
rotational and vibrational molecular modes, ionization, and
competing bond dissociation) and the conditions achieved
are much less extreme. Control of surfactants, supports, or
other reactants provides a facile route to a variety of metallic
nanomaterials (Fig. 7).2
Nanostructured metal particles were the first demonstration
of the application of chemical eects of high intensity ultrasound
for the preparation of nanomaterials.20 Ultrasonic irradiation of
solutions containing volatile organometallic compounds such
as Fe(CO)5, Ni(CO)4, and Co(CO)3NO produced porous, coral-like
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Fig. 6
The applications of sonochemistry to materials are diverse and rapidly expanding.
Fig. 7 The sonochemistry of volatile organometallics provides a versatile route

to a variety of nanostructured materials. Reprinted with permission from ref. 3.
Copyright 2010 John Wiley & Sons.
aggregates of amorphous metal nanoparticles.20,21 A classic example of this is the sonication of Fe(CO)5 in decane at 0 1C under Ar,
which yielded a black powder. The material was 496% iron, with
a small amount of residual carbon and oxygen present from the
solvent and CO ligands. SEM images revealed that the powder was
an agglomerate of 20 nm iron particles. If surfactants such as oleic
acid or polyvinylpyrrolidone were present in the solvent to
stabilize the particles then individual iron nanoparticles were
produced.22 These iron nanoparticles had a diameter of B8 nm
and were amorphous (measured by electron diraction).22
Magnetic studies indicated that these iron nanoparticles were
superparamagnetic. Bimetallic alloy particles have also been
prepared in this way. For example, sonication of Fe(CO)5 and
Co(CO)3NO led to the formation of FeCo alloy particles.23,24 The
composition was controllable by varying the ratio of the precursors
in the solution. Alloy nanoparticles typically exhibit superior
catalytic properties compared to monometallic nanoparticles.
The metal atoms decomposed from organometallic compounds during sonication are highly reactive and can react with
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Fig. 8 SEM images of (A) sonochemically synthesized MoS2 and (B) conventional MoS2. Reprinted with permission from ref. 25. Copyright 1998 American
Chemical Society.
other chemical substances in the solvent to form new materials.

Nanostructured MoS2, for example, was synthesized by the sonication of Mo(CO)6 with elemental sulphur in 1,2,3,5-tetramethylbenzene under Ar.25 MoS2 prepared sonochemically diers dramatically in morphology from conventional MoS2: conventional MoS2 is a
layered, plate-like material, while sonochemically synthesized MoS2
exhibited a spherical morphology with an average diameter of 15 nm
(Fig. 8). TEM examination revealed that sonochemically prepared
MoS2 contained more defects and showed many more edges,
although both MoS2 materials had the same interlayer distance of
0.62 0.01 nm. MoS2 has been frequently used as a hydrodesulfurisation catalyst in the petroleum industry to remove sulphur from
crude oil before combustion. Sonochemically prepared MoS2
exhibited substantially higher catalytic activity than conventional MoS2 for the hydrodesulfurisation of thiophene. The
increase in catalytic activity was attributed to the higher surface
area and more edges and defects found in the sonochemically
prepared MoS2.
The preparation of refractory nanomaterials remains problematic
because most high temperature routes lead to agglomeration of
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precursors or intermediate states during the synthesis. Sonochemical routes, however, produce the needed high temperatures
on the nanoscale in the localized hot spots of the collapsing
bubble. As a specific example, sonochemistry provides a convenient
approach to prepare nanostructured metal carbides that exhibit
excellent catalytic activity.26,27 Mo2C and W2C are particularly
interesting catalysts because they show catalytic activity similar to
platinum group metals, but their syntheses are challenging because
of the refractory nature of metal carbides. The sonication of
Mo(CO)6 or W(CO)6 in hexadecane leads to the formation of
amorphous metal oxycarbides. Removing oxygen by heating under
1 : 1 CH4/H2 leads to the formation of nanostructured Mo2C or W2C
as porous aggregates of small nanoparticles with surface areas of
130 m2 g1 and 60 m2 g1 for Mo2C and W2C, respectively. They
exhibit activities and selectivities similar to platinum for dehydrogenation reactions.26 In addition, these nanostructured metal
carbides show superior activity, selectivity, and stability for the
hydrodehalogenation of organic pollutants.27 Metal nitrides can
also be prepared by the sonication of metal carbonyl compounds
under a reductive gas mixture of NH3 and H2 at 0 1C.28
When a sacrificial template (e.g., microspheres of silica or
carbon) is present in the sonicated solution, the free metal atoms
produced by ultrasonic irradiation of volatile organometallic compounds can deposit onto the template to form dierent structured
materials. For example, ultrasonic irradiation of Mo(CO)6, sulphur,
and silica nanoparticles in isodurene under Ar forms MoS2-coated
silica nanoparticles.29 Replacing Ar with air and removing sulphur
from the system yields MoO3-coated silica nanoparticles. Etching of
the silica component by HF leaves hollow MoS2 or MoO3. These
hollow MoS2 nanoparticles had better catalytic activity toward
the hydrodesulfurization of thiophene than even sonochemically
prepared MoS2 nanoparticles due to the significantly increased
number of edge defects and improved accessibility to both inner
and outer surfaces of the hollow structures. Amusingly, the hollow
MoO3 spheres, which are initially amorphous, upon heating
crystallize into hollow single crystals.29
Ultrasonic irradiation of Fe(CO)5 in the presence of carbon
nanoparticles provided a facile method for the preparation of
hollow hematite.30 Carbon nanoparticles were used as a template
that spontaneously removes itself through combustion induced
by the rapid oxidation of the outer Fe shell upon exposure to air.
Porous Co3O4 was produced in a similar fashion when carbon
nanotubes were used as the template and Co4(CO)12 as the
precursor.31 Co3O4 prepared in this way was found to be an
excellent electrode material for lithium-ion batteries.
A sonochemical method has also been used to synthesize
single-walled carbon nanotubes via ultrasonic irradiation of a
solution containing silica powder, ferrocene, and p-xylene
(Fig. 9).32 In this synthesis, ferrocene was used as the precursor
for the Fe catalyst, p-xylene was used as a carbon precursor, and
silica powder provided nucleation sites for the growth of carbon
nanotubes. Ferrocene was sonochemically decomposed to form
small Fe clusters and p-xylene was pyrolyzed to carbon atoms
and carbon moieties. This approach provides a convenient
synthetic route for the preparation of carbon nanotubes under
ambient conditions. In addition, no extra purification steps
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Fig. 9 (A) Schematic illustration of the sonochemical preparation of singlewalled carbon nanotubes on silica powders. (B) SEM image of carbon nanotube
bundles on polycarbonate filter membrane. (C) HRTEM images of single-walled
carbon nanotubes within the bundles. Reprinted with permission from ref. 32.
Copyright 2004 American Chemical Society.
were needed in this process, which opens up the possibility for

large-scale ultrasonic synthesis of high-purity, single-walled
carbon nanotubes.
Ultrasonic irradiation of common organic solvents such as
CHCl3, CH2Cl2, and CH3I with HF-etched Si nanowires yielded
hydrocarbon materials with diverse structures (e.g., nanotubes
and nano-onions).33 The nanostructured SiHx on the Si nanowires served as a template for the nucleation of carbon species
formed from the pyrolysis of volatile organics inside the
collapsing bubbles.
B.
Nanomaterials prepared from nonvolatile precursors
Sonochemistry is also commonly used to prepare nanostructured noble metals when nonvolatile precursors are dissolved
in a volatile solvent (usually water or alcohols). In these cases,
sonolysis of the solvent vapour produces strong reductants that
have a number of advantages over traditional reduction techniques: no additional reducing agents are required, the
reduction rate is generally very fast, and very small nanoclusters
can be made in this way when suitable stabilizers are present.
Ultrasonic irradiation of water generates highly reactive H
and OH radicals which are responsible for redox chemistry.
These reactive radicals can further react with organic additives
(e.g., 2-propanol or ethanol) in the solution to generate secondary
radicals (R ) which can dramatically promote the reduction rate.
Overall, the process (including competing reactions) can be
summarized as follows:
H2O - H + OH
(1)
H + H - H2
(2)
H + OH - H2O
(3)
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OH + OH - H2O2
(4)
RH (volatile vapour) - R + H
(5)
RH + OH (or H ) - R + H2O (or H2)
(6)
Mn+ + nR (or H ) - M0
(7)
mM0 - Mm (M = noble metal)
(8)
Unlike metallic particles prepared from the sonication of volatile

organometallic compounds, which are typically amorphous,
materials produced from nonvolatile compounds are usually
well crystallized.
Nanostructured noble metals (e.g., Au, Ag, Pt, and Pd) can be
prepared by a large number of synthetic routes, including
controlled chemical reduction, solvothermal synthesis, photochemical reduction, and radiolytic reduction. Sonochemical
preparation also provides a facile approach for the production
of spherical metal nanoparticles.3440 A systematic study carried
out by Grieser et al. on the eect of ultrasound on the synthesis
of noble metal nanoparticles has shown that the particle size is
largely determined by solvent/surfactant properties: particle size
is inversely related to alcohol concentration and alkyl chain
length.34 This observation led to the conclusion that alcohol
molecules adsorbed to the surface of nuclei can limit the growth
of small nanoparticles. The other possible explanation for this
result is that more secondary radicals can form at higher alcohol
concentrations which leads to faster reduction rates which in
turn results in smaller and possibly more uniform particles.
Sequential sonochemical reduction of two dierent metallic
ions will result in bimetallic coreshell nanoparticles. For
example, the sonochemical reduction of a solution containing
both Au(III) and Pd(II) ions led to the formation of nanoparticles
with a Pd shell over an Au core.35 The coreshell structure is a
result of the dierence in reduction potential between Pd(II)
and Au(III) ions. When Au and Pd nanoparticles are formed
simultaneously, excess Au(III) ions will oxidize Pd nanoparticles
to form Au and Pd(II) ions. The Pd shell can only form once the
gold ions have all been reduced into nanoparticles. A similar
approach can be used to sonochemically prepare Au/Ag and
Pt/Ru coreshell particles.36,37
Sonochemical methods have also been developed to prepare
nonspherical nanoparticles. For example, gold nanorods have
been synthesized by the sonochemical reduction of HAuCl4 in
the presence of AgNO3, CTAB, and ascorbic acid.38 The solution
pH influences the aspect ratio of the gold nanorods: as the pH
of the solution increases, the average aspect ratio of the gold
nanorods decreases. Ultrasound-induced reduction of HAuCl4
onto pre-synthesized gold seeds using polyvinylpyrrolidone
(PVP) as a stabilizing polymer leads to the formation of monodispersed gold nanodecahedra.39 This sonochemical method can
significantly increase the yield and reproducibility. Ag nanoplates
have also been synthesized by a similar ultrasound-assisted
Ostwald ripening process using Ag nanoparticles as seeds.40 These
platelike nanostructures served as templates to fabricate ringlike
metal structures via a simple displacement reaction under
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ultrasonic irradiation. Ag nanowires and nanorods have also

been prepared by sonicating suitable Ag precursors.
Polymers or small molecules can act as structure directing
agents as well as stabilizers. Ultrasonic irradiation of HAuCl4
solution containing a-D-glucose produced gold nanobelts with a
width of 3050 nm and a length of several micrometres.41 These
gold nanobelts are formed through 3 steps: (1) formation of
gold nanoparticles via sonochemical reduction, (2) aggregation
and room-temperature temperature sintering of gold nanoparticles directed by a-D-glucose, and (3) further growth along
the Au[111] direction with recrystallization finally yielding the
isolated single-crystalline gold nanobelts.
Highly fluorescent, stable, and water-soluble Ag nanoclusters (diameter less than 2 nm) have been successfully prepared
by sonication of aqueous AgNO3 solutions with dissolved polymethylacrylic acid (PMAA) (Fig. 10).42 The charged carboxylate
groups of PMAA can stabilize clusters of Ag atoms in solution
and prevent further growth of nanoclusters to form large
nanoparticles. The optical and fluorescence properties of these
Ag nanoclusters can be controlled by varying synthetic conditions, e.g., sonication time, stoichiometry of the carboxylate
groups relative to Ag+, and the polymer molecular weight. Ag
nanoclusters, as a new kind of nanoparticle fluorophore, are
likely to find widespread applications in bioimaging, chemical
and biosensing and single-molecule studies.
Fig. 10 (A) Fluorescence emission spectra of Ag nanoclusters prepared by the

sonochemical method with dierent durations of sonication time, indicated in
minutes (inset: vial containing a solution of the Ag nanoclusters illuminated by a
365 nm UV lamp). (B) TEM images of as-prepared Ag nanoclusters after 90 min
sonication (inset shows a single magnified Ag nanocluster). Reprinted with
permission from ref. 42. Copyright 2010 American Chemical Society.
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Fig. 11 SEM images of (A) typical trigonal Se nanowires synthesized by sonication of amorphous selenium grown in ethanol at room temperature and
(B) grown from amorphous Se colloids in ethanol without sonication. Reprinted
with permission from ref. 43. Copyright 2003 American Chemical Society.
The sonochemical reduction of nonvolatile precursors in

solution is not limited to noble metals. For example, trigonal Se
nanowires were prepared by the sonication of amorphous Se
colloids in alcohol solvents without templates or surfactants
(Fig. 11).43 Nanocrystals of trigonal Se were nucleated sonochemically and acted as seeds for the growth of Se nanowires
through a solid-solution-solid transformation mechanism driven
thermodynamically: amorphous Se has a higher free energy than
trigonal Se.
Various metal oxides and metal chalcogenides have also
been prepared by sonochemical methods with nonvolatiles.4446
A typical synthesis of these types of materials involves the
sonication of a solution containing a metal salt and an oxygen
or chalcogen source (e.g., air for oxygen, thiourea for sulphur,
selenourea for selenium, or sometimes, a sulphate or selenate).
Reactive species such as reactive radicals or atoms (O or S ) can
react with metal ions in the solution to form metal oxides or
metal chalcogenides. If proper structure directing agents are
used, dierent nanostructured materials (e.g., hollow spheres,
nanorods, nanowires, or nanocubes) can be obtained. For example,
ultrasonic irradiation of CdCl2, NaSeSO3, and ammonia leads to the
formation of hollow CdSe spheres.44 CdCl2 was hydrolysed under
the basic conditions to form Cd(OH)2 which acted as an in situ
template for the sonochemical formation of hollow structures. This
process can be written as follows:
H2O - H + OH
(9)
2H + SeSO32 - Se2 + 2H+ + SO32

Cd(OH)2 + Se
- CdSe + 2OH
nCdSe - (CdSe)n
(10)
(11)
(12)
Hetero-structured materials such as coreshell SnO2/CdS

and ZnO/CdS have also been prepared via sonochemical
deposition of metal sulphide onto metal oxides.45 In a similar
fashion, by exploiting the hydrogen radicals formed from
sonolysis of water vapor inside the collapsing bubbles, copper
hydride (CuH) can be produced via ultrasonic irradiation of a
copper(II) aqueous solution.46
As a synthetic tool, sonochemistry can deposit nanoparticles
formed in situ onto pre-existing substrates (e.g., polystyrene
spheres, silica particles, carbon nanotubes, or a polymer
matrix).4749 Graphene has emerged as a new 2D material with
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unique electrical, thermal, and mechanical properties. Catalyst

assemblies of nanostructured materials with exfoliated, singlelayer graphene (often prepared sonochemically, as discussed
later) have shown great promise for a wide range of applications including sensors, fuel cells, lithium-ion batteries, photocatalysts, and fuel cells. Ultrasonic irradiation of graphene
oxide with HAuCl4 in water produced well-dispersed reduced
graphene oxide/Au composites by simultaneous or sequential
reduction procedures.50 The formation of reactive OH and H
radicals via sonolysis of water vapour inside collapsing bubbles
is responsible for the formation of reduced graphene oxides
and the reduction of Au(III) to Au nanoparticles (eqn (1)(7)).
Aligned nanostructures can be achieved with the help of
ultrasound. For example, vertically aligned ZnO nanorods were
prepared on substrates such as Zn sheets, Si wafers, glass, and
polycarbonate membranes by sonicating a precursor solution
containing Zn2+.51 Ultrasonic irradiation rapidly induces the
anisotropic growth of ZnO along the (0001) direction on
the substrate. The alignment is presumed to be due in part to
the relative depletion of Zn2+ concentration at the base of the
growing rods relative the tops of the rods. Oxygen atoms,
hydroxyl radicals or hydroperoxyl (HO2) radicals formed by the
sonication of water in air are thought to be responsible for the
formation of these ZnO rods. Compared to a conventional
hydrothermal process, the growth rate of ZnO is increased by
10 fold, with an average growth rate of B500 nm h1.
3. Physical eects of ultrasound for

nanomaterials synthesis
The most important physical eects of high intensity ultrasound
arise from the high-speed jets and intense shock waves induced by
cavitation. They have been frequently used to prepare emulsions,
agglomerate malleable materials, break down friable materials,
modify solid surfaces, and exfoliate layered materials. Enhanced
mass transfer as a consequence of acoustic streaming and bulk
thermal heating are other physical eects of high intensity
ultrasound.
A good example of exploiting the physical eects of ultrasound is the enhancement of intercalation of guest substances
into layered materials first developed by Green, Suslick and
co-workers.52 In more recent work, graphite, with its layered
planar structure, can accommodate in between each graphene
layer guest molecules or atoms to form graphite intercalation
compounds, but the formation of intercalation compounds is
usually a very slow process. Ultrasonic irradiation, however, can
dramatically increase the reaction rate.53 For example, potassium intercalated compounds (KC8) can be prepared by the
sonication of graphite with potassium under an Ar atmosphere in
3 minutes while normal preparation methods require 18 hours
via a solid state reaction at high temperature under an inert
atmosphere. H2PtCl6 can also be intercalated into graphite layers
to prepare Pt nanoparticles intercalated in graphite after exposure
to an H2 gas stream.54 The sonication of potassium intercalated
graphite in ethanol can generate carbon nanoscrolls (Fig. 12).55
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Fig. 12 (A) Schematic illustration of the intercalation and exfoliation process to

prepare carbon scrolls. TEM images of (B) a thin layer of graphite sheets in the
process of scrolling, (C) an isolated carbon nanoscrolls with open ends, and (D) a
bundle of scrolled carbon nanosheets. Reprinted with permission from ref. 55.
Copyright 2003 AAAS.
The conversion eciency is very high, up to B80%, compared

to a reaction in the absence of ultrasound, which results in very
few nanoscrolls. The reason for the formation of carbon
nanoscrolls is not fully understood, but ultrasound provides
the necessary mechanical energy to overcome the van der Waals
force between each graphene layer. The individual exfoliated
graphene layers can then fold via intralayer interactions to
reach a stable structure in the solvent.
Ultrasound has become a formidable tool for the chemical
preparation of single and few layer graphene. In a typical
synthesis of graphene oxide, pristine graphite is oxidized by
Hammers method to form graphite oxide, which has an
increased interlayer distance relative to graphite and the van
der Waals force is consequently weaker. After mild sonication
(e.g., bath sonication is sucient), single-layered graphene oxides
can be produced which can then be chemically reduced to graphene.
A more straightforward method for the preparation of graphene is
the direct liquid-phase exfoliation of graphite by sonication. To
obtain high yields of exfoliated graphenes from graphite, the
surface energy of the solvent must match the surface energy of
graphite, 4050 mJ m2. Sonication of graphite in suitable solvents
(e.g. N-methyl-pyrrolidone (NMP)) can lead to the formation of single
layer and few-layer graphenes.56 Ultrasound is also frequently used
to disentangle single-walled carbon nanotubes, which usually form
bundles due to the van der Waals force.
This approach can be generalized to other layered materials
such as MoSe2, MoTe2, MoS2, WS2, TaSe2, NbSe2, NiTe2, BN,
and Bi2Te3, all of which can be exfoliated in the liquid phase to
prepare single-layered nanosheets (Fig. 13).57 Ultrasound is a
broadly useful tool for overcoming the attractive forces between
individual layers to break 3D layer-structured materials down to
2D planar structures.
The impact of ultrasonic shock waves on pre-existing particles
in a liquid is also an interesting use of the physical eects of
ultrasound. For instance, high intensity ultrasound can drive
metal microparticles suspended in liquid slurries into one another
at high speeds (hundreds of metres per second) to induce local
melting at the point of collision and consequent agglomeration
(Fig. 14).16,17 This can only happen with metals with relatively low
melting point (e.g., Sn, Zn, Cr, and barely Mo). If the melting points
of the metal is higher than B3000 K, no melting at the point of
impact occurs. Furthermore, agglomeration of metal particles
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Chem. Soc. Rev., 2013, 42, 2555--2567
Fig. 13 TEM images of individual nanosheets. (A to C) Low-resolution TEM

images of flakes of BN, MoS2, and WS2, respectively. (D to F) High-resolution TEM
images of BN, MoS2, and WS2 monolayer (Insets) Fast Fourier transforms of the
images. Reprinted with permission from ref. 57. Copyright 2011 AAAS.
Fig. 14 Eects of ultrasonic irradiation on slurries of fine Zn powder (5 mm

diameter, roughly spherical). (A) SEM before ultrasonic irradiation. (B) Dense
agglomeration after 90 min sonication of 2% w/w decane slurry at 20 kHz,
50 W cm2, 283 K, where agglomerates are made from B1000 of the initial
particles and loadings up to 50% w/w show similar results. The same magnification is used in both images. Reprinted with permission from ref. 17. Copyright
2004 American Chemical Society.
occurs only over a fairly narrow range of radius in the regime

of a few microns. Neither particles too large nor too small will
be accelerated to a sucient velocity to induce local melting
and consequent agglomeration (Fig. 15).
Such interparticle collisions during ultrasonic irradiation of
slurries of high temperature superconductors can significantly
improve their properties.58,59 For example, the superconducting
properties of Bi2Sr2CaCu2O8+x are significantly improved after
sonication as a slurry in decane due to the enhancement of
intergrain coupling resulting from interparticle collisions.58 Intergrain coupling controls the critical magnetic field (Jc) that limits the
fields that can be formed with Bi2Sr2CaCu2O8+x superconductors.
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Fig. 15 Calculated velocities of interparticle collisions of Zn powder during

ultrasonic shock waves as a function of particle radius. The critical velocity
necessary for collisional agglomeration determines the particle size range
over which agglomeration will occur. Reprinted with permission from ref. 17.
Copyright 2004 American Chemical Society.
Ultrasound can also be used to promote the diusion of

dopant ions into spherical nanoparticles. For example, high
intensity ultrasound is used to prepare Mg2+ doped ZnO
nanoparticles with tuneable photoluminescence (from yellow
to blue, Fig. 16).60 The quantum yield of these Mg2+ doped ZnO
nanoparticles is very high, 460% under optimal conditions.
XRD and HRTEM results indicate that no MgO phase exists in the
ZnO nanoparticles. Ultrasonic irradiation of a slurry containing
Au colloids and TiO2 particles can lead to the formation of Au
nanoparticles intercalated into a mesoporous TiO2 structure
which shows enhanced photocatalytic properties.61
The microjets and shock waves produced by high intensity
ultrasound near solid surfaces can also cause physical changes
on the surfaces of particles and substrates. For instance, high
intensity ultrasound has been applied to improve anticorrosion
surface coatings. Generally, even pure aluminium metal is
coated by a few nm thick oxide layer. This layer is not able to
Fig. 16 Photographs (under UV light) of ethanol solutions (upper) and dry

powders (lower) of Mg/ZnO nanoparticles prepared by ultrasonic irradiation of
ZnO with Mg2+ with dierent Mg/Zn ratios. Reprinted with permission from
ref. 60. Copyright 2009 John Wiley & Sons.
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protect fully against corrosion agents and is often not strongly
adhered to the underlying metal. The corrosion protection and
adhesion properties, however, can be improved via ultrasonic
treatment.62 After ultrasonic irradiation, the existing oxide layer
is removed and a newly active oxide layer forms that has been
shown to exhibit superior resistance to corrosion.
Ultrasonic irradiation can also improve solgel syntheses, a
versatile technique for the preparation of nanostructured metal
oxides. Application of ultrasound during a solgel process can
accelerate the hydrolysis process and create metal oxides with
narrower size distributions, higher surface area, and improved
phase purity. For example, TiO2, ZnO, CeO2, MoO3, V2O5, and
In2O3 have all been prepared by the ultrasonic irradiation of
their respective precursor solutions.63,64 TiO2 nanoparticles
prepared by ultrasonic irradiation of the precursor solution
are more photocatalytically active than commercial TiO2 nanoparticles.63 The increase in photocatalytic activity is attributed
to the improved crystallinity of TiO2 which is achieved due to
accelerated hydrolysis under sonication.63 Ultrasound can also
induce the formation of unique morphologies during the
synthesis of nanostructured metal oxides in the presence of
soft templates. For example, hollow PbWO4 spindles were
prepared from the sonication of a solution of Pb(CH3COO)2,
NaWO4, and P123 (a Pluronic block copolymer, EO20PO70EO20,
Mavg = 5800).65 In the absence of ultrasound, however, only
solid particles were obtained. It was argued that ultrasound
played an important role in the transformation of P123 micelles
into hollow micelle aggregates which led to the formation of
the hollow spindle structure.
The power of the physical eects of high intensity ultrasound is further illustrated by mechanochemical reactions of
polymers, which include force-induced scission of covalent
bonds. It has been well known since the 1950s that ultrasonic
irradiation of solutions of high molecular weight polymers
(both biomolecular and synthetic) results in chain scission
and macroradical production.66 More recently, the incorporation
of mechanically sensitive chemical groups (mechanophores) into
a polymer chain has made it possible to illustrate the mechanical
forces present during exposure to ultrasound.67 Sonication
accelerates rearrangement reactions with a bias towards reaction pathways that yield molecules not necessarily obtained
from purely thermal or light-induced reactions.67 For example,
when 1,2-disubstituted benzocyclobutene is incorporated into
a polymer chain and undergoes an ultrasonically-triggered
electrocyclic ring opening process the same products are
formed regardless of whether the original molecule was cis or
trans (Fig. 17). If the reactions were initiated by light or heat
alone, dierent products would form depending on the initial
isomer. Thus, the mechanical force induced by ultrasound can
alter the shape of the potential energy surfaces so that otherwise disfavored reactions can proceed under mild conditions.
Ultrasound oers a way to access reaction pathways that may
dier dramatically from those achieved by simply changing
chemical or physical parameters. If stress-sensitive and cleavable
groups are integrated in the polymer chain, sonication can result
in the precise scission of the polymer chains. Some weak covalent
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ultrasound for materials synthesis. In sonochemistry, ultrasound directly induces chemical reactions; while in USP, sonication does not produce chemical species and therefore does
not cause chemical reactions. In fact, ultrasonic vibrations at
the liquid surface are used to generate isolated microdroplets
due to surface capillary waves.3 These microdroplets act as
individual microreactors with a series of thermally driven reactions occurring inside microdroplets as they flow through
a heated oven. The applications of USP for nanostructured
materials synthesis have been reviewed elsewhere.3
4. Combined chemical and physical eects

for ultrasonic synthesis of nanomaterials
Fig. 17 Predicted intermediates of benzocyclobutene based on dierent activation mechanisms. Top: light activation induces only disrotary (dis) ring opening.
Middle: heat activation induces only contrarotary (con) ring opening. Bottom:
stress (ultrasound) causes dis or con ring opening depending on initial isomer.
Reprinted with permission from ref. 67. Copyright 2007 Nature Publishing Group.
bonds such as peroxide and azo bonds, strained rings, and weak
coordinative bonds (e.g., palladiumphosphorus bonds) can be
cleaved by ultrasound,6871 and even the click reaction can be
unclicked within a polymer chain.72
Ultrasound also has eects on the process of crystallization
(through increased nucleation, enhanced mass transport to the
crystal surface, and sonofragmentation of larger crystals).73 Sonication has been used to prepare nanostructured organic crystals,
although reports of the formation of nanosized crystals in this
area are uncommon; typical crystals produced in this way are of
micron scale.73 One example of the application of ultrasound to
the preparation of nanocrystals is the preparation of cocrystals of
2(resorcinol) 2(4,4 0 -bpe), which can produce nanocrystalline
cocrystals that exhibit single-crystal-to-single-crystal reactivity.74
Compared with conventional reprecipitation methods, crystals
obtained via sonochemistry were smaller and more uniform in
size. Nanosized organic crystals of a self-assembled hexamer have
also been prepared via an ultrasound-induced crystallization
process. Nanosized hollow rhombic-dodecahedral crystals of
the C-methylcalix[4]resorcinarene hexamer were achieved with
rapid nucleation of a crystalline phase.75 The mechanism for the
formation of the hollow organic crystals is attributed to a reversed
crystal growth mechanism heretofore described only in the
synthesis of inorganic-based materials.
Broadly speaking, ultrasonic spray pyrolysis (USP) might
also be regarded as an example of using physical eects of
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Chem. Soc. Rev., 2013, 42, 2555--2567
Under certain conditions, both the chemical and physical

eects of high intensity ultrasound can play a synergistic role
in the synthesis of nanomaterials. The application of the
physical eects of ultrasound on the preparation of graphene
was described in Section 2, but the chemical eects of ultrasound can also be exploited to aid in the preparation of
functionalized graphenes. Recent work has shown that the
use of a reactive solvent, such as styrene, that can be sonochemically activated allows for the relatively facile production
of polymer functionalized single and few-layer graphenes in a
single step.76 During ultrasonic irradiation of graphite in
styrene, polystyrene radicals will form and attack the surface
of the exfoliated graphenes to form functionalized graphenes.
Alternatively, the surface of graphite may first be functionalized
by the radicals followed by exfoliation and further functionalization
of the newly exposed graphene face will occur (Fig. 18). TEM images
of graphenes prepared in this way are shown in Fig. 19. Sonication
of a solution containing poly(vinyl alcohol) and graphite also led
to the formation of polymer functionalized graphenes.77 The
functionalization was achieved via sonochemical degradation of
poly(vinyl alcohol) to form macroradicals which then grafted
onto graphene surfaces.
Another notable example of the application of both chemical
and physical eects of high intensity ultrasound in materials
synthesis is the preparation of protein microspheres. Sonication of a protein solution (e.g., serum albumins) led to the
formation of microcapsules which can contain gas or nonaqueous
Fig. 18 Schematic illustration of the mechanochemical eects of ultrasound for

the synthesis of polymer functionalized graphenes. Reprinted with permission
from ref. 76. Copyright 2011 American Chemical Society.
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Fig. 19 TEM images of (A) single-layer graphene and (B) trilayer graphene with
SAED insets confirming single-layer and few-layer graphenes, respectively.
Reprinted with permission from ref. 76. Copyright 2011 American Chemical Society.
Tutorial Review
sonography (e.g., echocardiography) has become standard.83
Protein microspheres have also been developed as 19F-MRI
contrast agents,84 as in vivo MRI temperature probes,85 as
optical coherence tomography contrast agents,86 for encapsulation and drug release,8789 and as multifunctional, multimodal
cancer imaging contrast agents.90
The combination of chemical and physical eects of ultrasound
can also be applied to prepare organic latex beads in a one-pot
fashion. Through intense turbulence, ultrasound will create an
emulsion of organic monomer in an aqueous medium. The radicals
formed by sonolysis of water can diuse into the organic phase to
initiate the polymerization process. No additional initiators are
required in this approach. In this method, fluorescent or magnetic
substances can be incorporated into the latex particles to prepare
functional latex beads.91,92 For example, magnetic latex beads with a
high content of magnetic nanoparticles have been prepared by
ultrasonic irradiation of an emulsion of magnetite nanoparticles,
surfactants, water and a reactive monomer.92 Short sonication of
this solution results in the formation of an emulsion of monomer
loaded with magnetite nanoparticles stabilized by surfactants in the
aqueous phase. Continuous sonication initiates the polymerization
of the monomers to form latex particles.
5. Conclusions
Fig. 20 SEM images of sonochemically prepared protein microspheres before and

after nanoparticle functionalization by layer-by-layer adhesion: upper left, native
microspheres as prepared by sonication of bovine serum albumin and upper right,
close-up of the surface; lower left, silica-coated microspheres using a RGD polylysine
peptide to reverse surface charge and lower right, close-up of its surface. Reprinted
with permission from ref. 80. Copyright 2006 American Chemical Society.
liquid and whose surfaces are easily modified (Fig. 20).7880 The
mechanism responsible for the formation of protein microspheres involves two acoustic phenomena: emulsification
(a physical eect) and cavitation (and the subsequent chemical
eects). Sonication creates an emulsion with proteins in the
interface of two liquid phases. However, emulsification alone is
not enough to prepare stable protein microspheres. Radicals
(e.g., HO2 ) produced via the sonolysis of water induce the
cross-linking of the disulphide bonds between cysteine amino
acid residues. The protein microspheres can also be modified
after sonochemical preparation, for example with conjugation of
cancer-cell selective ligands (e.g., folate, monoclonal antibodies,
RGD peptides, mercaptoethane sulphonate) to their surface.80,81
Similar procedures can be used to prepare polysaccharide-based
microspheres, for example, chitosan microspheres have been
prepared in a single-step using sonochemical method.82 The
intermolecular imine cross-linking is important to the stabilization of the chitosan microspheres.
These protein microspheres have a wide range of clinical
applications. Their use as echo contrast agents for improved
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High intensity ultrasound is responsible for a number of physical

and chemical eects that are conducive to the preparation or
modification of nanomaterials. The diverse mechanisms of action
make it a powerful tool relevant to a large number of topics of
current interest, including graphene, polymers, metal and metal
oxide catalysts, crystallization, and anisotropic materials. With
simple variations of reaction conditions and precursor compositions, a myriad of nanostructured materials with controlled
morphologies, structures, and compositions have been successfully
prepared by the application of high intensity ultrasound.
Acknowledgements
This work was supported by the NSF (DMR 09-06904). KSS would
like to dedicate this paper to his mentors, Professors James P.
Collman, John I. Brauman, and Robert G. Bergman, on the
occasion of their 80th, 75th, and 70th birthdays, respectively.
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